CN105597143B - A kind of method that pure water mutually prepares styptic powder - Google Patents
A kind of method that pure water mutually prepares styptic powder Download PDFInfo
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- CN105597143B CN105597143B CN201610067467.7A CN201610067467A CN105597143B CN 105597143 B CN105597143 B CN 105597143B CN 201610067467 A CN201610067467 A CN 201610067467A CN 105597143 B CN105597143 B CN 105597143B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
- A61L24/08—Polysaccharides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/04—Materials for stopping bleeding
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Abstract
The present invention relates to styptic powder technical field, in particular to method that a kind of pure water mutually prepares styptic powder: starch being mixed with acetone and is soaked for a period of time, and elutes drying afterwards, and the gelatinization of starch solution prepares cross-linking agent solution, cross-linking reaction, cleaning purifying, screening packaging.Simple process, pure water phase technical process is fairly simple, reduces some reaction systems, saves the production cost more than half；Hemostasis granules rate of water absorption is fast, can preferably absorb wound blood quickly, can play the role of stopping blooding rapidly in practical application；Toxicity is smaller, and biocompatibility is more preferable, because, in product cleaning without using organic solvents such as ethyl acetate, the residual of ethyl acetate is not present in final product without oil phase in reaction process.The cost of production has also further been saved simultaneously.
Description
Technical field
The present invention relates to styptic powder technical field, in particular to method that a kind of pure water mutually prepares styptic powder.
Background technique
It mainly include glutin, fiber egg currently, having developed the wound hemostasis material of various new perhaps both at home and abroad
White glue, soluble stanching gauze, zeolite and degradable hemostatic material etc..(1) glutin includes gelfoam, microcrystalline collagen
Gelfoam etc. is coagulated with increasing, such hemostatic material anthemorrhagic speed is slow, to the drawing ability and the surface of a wound of the blood constituents such as blood platelet
It organizes adhesive force poor, is easily broken.(2) Fibrin Glue has clinically been answered extensively as surface of a wound hemostasis binding material
With.It as the shortcoming of wound first-aid supply be it is at high cost, human body or animal blood borne disease may be brought to infect, use
More complex, anthemorrhagic speed is slowly and low etc. to big angiorrbagia success rate of hemostasis.(3) soluble stanching gauze belongs to carboxymethyl
Sodium cellulosate class hemostatic material can complete hemostasis in 2-8 minutes, and bleeding stopping period is longer, very poor to the swift and violent person's effect of bleeding, no
It is suitble to separately as wound hemostasis material.(4) about zeolite: it is reported that U.S. army makes in Afghan War and the war in Iraq
War wound wound is stopped with the styptic sponge (trade name Quickclol) that a u s company (Z-Medica) produces
Blood, the material main component are a kind of zeolites (zeolite).Material hemostasis meeting heat release, so hurting in large-area hemorrhage
Using tissue thermal damage can be caused on mouthful, when in addition stopping blooding to arterial hamorrhage, it is necessary to wrap up a kind of pressurization again in its outer layer
Auxiliary material in this way can have some impact on affected part blood circulation.
It includes that (1) takes one that CN1947800A, which discloses a kind of hemostatic micro-granules and its preparation method, the preparation method of the hemostatic micro-granules,
Determine the potato starch of unit of weight, 10-50 times of distilled water is added, in starch solution sodium hydroxide solution tune after stirring sufficiently
Whole pH value is 8.0-10.0；Or the constant temperature in 50-70 DEG C of water-bath of the starch solution after distilled water will be added to be gelatinized, after gelatinization completely
Starch solution in be added dropwise sodium hydroxide solution, adjustment pH value is 8.0-10.0；(2) it produces paraffin oil-starch mixed solution: taking
Span80 emulsifier, atoleine, mixing, stir 5-30 minutes in 50-70 DEG C of thermostat water bath, are then added to step
(1) it in starch solution, stirs 5-30 minutes, the envelope-bulk to weight ratio of paraffin oil and potato starch, ml/g, is 25-200:1；
The weight ratio of span80 emulsifier and potato starch, g/g are 0.1-2.5:1；(3) crosslinking Treatment: above-mentioned paraffin oil-starch
The epichlorohydrin of certain volume unit is added in mixed solution, is stirred to react 1-10 hours, the volume of epichlorohydrin and potato starch
Weight ratio, mg/g are 0.05-2.0:1；(4) prepare hemostatic micro-granules: above-mentioned reactant stratification takes lower layer's milky white liquid,
Ethyl acetate liquid separation is added, additional amount is 4-5 times of lower layer's milky white liquid, stirring；Stratification again takes lower layer's milky liquid
Body is added 2-3 times of washes of absolute alcohol, is stirred for, is then filtered by vacuum to moisture pump, and obtained solid powder is through dry
Getting the product is packed after dry, screening.
Rate of water absorption using hemostatic micro-granules made from this method is lower, and preparation process is more complicated, the cleaning of product
Purifying is needed using a large amount of ethyl acetate, the more difficult removal of dissolvent residual.
Summary of the invention
In order to solve big, the obtained styptic powder bleeding stopping period length of complex process, solvent consumption in styptic powder preparation process
Problem, that this application provides a kind of preparation processes is simple, reacts in water phase, post-processes good pure of simple, haemostatic effect
The method that water phase prepares styptic powder.
The present invention is achieved by the following measures:
A kind of method that pure water mutually prepares styptic powder, comprising the following steps:
(1) pre-treatment of starch:
Starch is mixed with acetone and is soaked for a period of time, elutes drying afterwards；
(2) gelatinization of starch solution:
After mixing by starch and water dry in step (1), Heat Gelatinization adjusts pH value after cooling；
(3) preparation of cross-linking agent solution:
Crosslinking agent is taken, surfactant and water is added, emulsification is uniform to obtain cross-linking agent solution；
(4) cross-linking reaction
Cross-linking agent solution is poured into the gelatinized starch of step (2) and is reacted；
(5) cleaning purifying, screening packaging
Reaction solution is dry after being cleaned with ethyl alcohol, screening dress sample.
The mixed weight ratio of the preparation method, preferred starch and acetone is 1:0.25-2.5, preferably 1:0.4-
0.75。
The preparation method, the weight ratio of starch and water is 1:5-1:30, preferably 1:20, pH value in preferred steps (2)
8-11, preferably 9-11.
The weight ratio of the preparation method, preferred starch and crosslinking agent is 5-80:1, preferably 25-80:1, preferably 50-
80:1 or 25-50:1；The weight ratio of surfactant and crosslinking agent is 0-1:4-8, preferably 1:4-8.
The preparation method, the reaction time is 2-6 hours, 50-75 DEG C of temperature range, preferably 60- in preferred steps (4)
70℃。
The preparation method, preferably crosslinking agent are epoxychloropropane, formaldehyde, glutaraldehyde or 1,4 butanediol glycidols
Ether.
The preparation method, preferred starch are potato starch, cornstarch or amylopectin.
The preparation method, preferred surfactant are Tween 80, span80, polysorbate60, span60 and dodecyl
One or more of benzene sulfonic acid sodium salt, preferably span80 and polysorbate60 mass ratio 9:1.
Beneficial effects of the present invention:
1, simple process, pure water phase technical process is fairly simple, reduces some reaction systems, saves the production more than half
Cost；
2, hemostasis granules rate of water absorption is fast, can preferably absorb wound blood quickly, can play in practical application fast
The effect of short stopping blood；
3, toxicity is smaller, and biocompatibility is more preferable because in reaction process without oil phase, product cleaning when without using
The residual of ethyl acetate is not present in the organic solvents such as ethyl acetate, final product.Production has also further been saved simultaneously
Cost.
Specific embodiment
In order to better understand the present invention, it further illustrates combined with specific embodiments below.
Embodiment 1:
After mixing in 1:20 ratio by dry potato starch 20g and water, 70 DEG C of Heat Gelatinizations adjust after cooling
PH value is 9.Crosslinking agent epoxychloropropane 0.4g is taken, surfactant span80 0.1g and water 5ml is added, is added after emulsifying uniformly
Enter into the starch solution of gelatinization, 60 DEG C are reacted 6 hours, stop heating, reaction was completed.Reaction solution is poured into dehydrated alcohol and is sunk
It is precipitated, dry after cleaning 3 times, screening dress sample.
Embodiment 2:
Acetone 8g is added in potato starch 20g, impregnates washing and drying after 1h, treated starch is according to embodiment 1
Method is tested.
Embodiment 3:
Sodium hydroxide solution 100g is added in potato starch 20g, impregnates washing and drying after 2h, treated starch according to
The method of embodiment 1 is tested.
Embodiment 4:
Sodium dodecyl benzene sulfonate aqueous solution 100g is added in potato starch 20g, washing and drying after 2h is impregnated, after processing
Starch tested according to the method for embodiment 1.
Embodiment 5: hemostasis trial
Product obtained in embodiment 1,2,3,4 is subjected to animal experiment:
Hemostasis duration measuring method:
Animal packet: selecting healthy SD rat male and female each 25, is randomly divided into totally 5 groups of a, b, c, d, blank control, every group equal
10 animals, half male and half female.
Method: after every rat tail vein of the crosscutting rat of sharp cutter away from tail point portion about 8cm, each administration group is given
Different groups of other test samples are given, blank control group does not give any processing.The bleeding time of every rat is recorded with stopwatch and is stopped
The blood time calculates hemostasis duration (bleeding stopping period-bleeding time, unit: s).
Data processing: each administration group rat hemostasis duration is compared with blank control group carries out statistics, to judge drug
Effect, stop blooding duration with mean ± standard deviation () indicate.
Rat hemostasis trial calculated result
(compared with the control group :-P>0.05 ,+P<P<0.01 0.05, *)
Wherein N is experimental animal number of cases；M is duration of averagely stopping blooding, unit s.
It can be seen that the product haemostatic effect that starch that acetone treatment is crossed obtains after being reacted from the result of animal experiment
It is relatively good.
Embodiment 6:
It takes each 20g of 6 parts of potato starch that acetone is added and is followed successively by 0g, 5g, 10g, 15g, 25g, 50g, washed after impregnating 1h
Dry, after mixing in 1:20 ratio by dry starch and water, 70 DEG C of Heat Gelatinizations, it is 9 that pH value is adjusted after cooling.Take friendship
Join agent epoxychloropropane 0.4g, surfactant span80 0.1g and water 5ml is added, the shallow lake of gelatinization is added to after emulsification uniformly
In powder solution, 60 DEG C are reacted 6 hours, stop heating, reaction was completed.Reaction solution is poured into dehydrated alcohol and is separated out, is cleaned 3 times
After dry, screening dress sample.Obtained product carries out haemostatic effect test,
| Amount/g of acetone is added | 0 | 5 | 10 | 15 | 25 | 50 |
| Stop blooding duration/s | 164.00 | 113.20 | 105.50 | 112.70 | 118.60 | 119.20 |
Embodiment 7:
Acetone 10g is added in amylopectin 20g, washing and drying after 1h is impregnated, by dry starch and water in 1:20 ratio
After mixing, 70 DEG C of Heat Gelatinizations, it is 9 that pH value is adjusted after cooling.Crosslinking agent glutaraldehyde (concentration 25%) 1g is added, 70 DEG C anti-
It answers 6 hours, stops heating, reaction was completed.Reaction solution is poured into dehydrated alcohol and is separated out, dry after cleaning 3 times, screening dress
Sample.Obtained product carries out haemostatic effect test, and stop blooding duration how many 110.20s, and haemostatic effect is preferable.
Embodiment 8:
Acetone 10g is added in cornstarch 20g, washing and drying after 1h is impregnated, by dry starch and water in 1:20 ratio
After mixing, 70 DEG C of Heat Gelatinizations, it is 10 that pH value is adjusted after cooling.Be added crosslinking agent formalin (concentration 40%) 1g, 70 DEG C
Reaction 6 hours stops heating, and reaction was completed.Reaction solution is poured into dehydrated alcohol and is separated out, dry after cleaning 3 times, screening dress
Sample.Obtained product carries out haemostatic effect test, and stop blooding duration how many 112.00s, and haemostatic effect is preferable.
Embodiment 9:
Acetone 8g is added in potato starch 20g, washing and drying after 1h is impregnated, by starch after drying and water in 1:20 ratio
After mixing, 70 DEG C of Heat Gelatinizations, it is 11 that pH value is adjusted after cooling.Crosslinking agent epoxychloropropane 0.8g is taken, it is living that surface is added
Property agent span80 0.1g and water 5ml, emulsification uniformly after be added in the starch solution of gelatinization, 60 DEG C react 6 hours, stop plus
Heat, reaction was completed.Reaction solution is poured into dehydrated alcohol and is separated out, dry after cleaning 3 times, screening dress sample.Obtained product into
Whereabouts blood measure of merit, stop blooding duration how many 110.30s, and haemostatic effect is preferable.
Embodiment 10:
Acetone 8g is added in potato starch 20g, washing and drying after 1h is impregnated, by starch after drying and water in 1:20 ratio
After mixing, 70 DEG C of Heat Gelatinizations, it is 11 that pH value is adjusted after cooling.Crosslinking agent epoxychloropropane 0.8g is taken, it is living that surface is added
Property agent compounding span80 and polysorbate60 (9:1) total 0.1g and water 5ml, be added in the starch solution of gelatinization after emulsification is uniform,
60 DEG C are reacted 6 hours, stop heating, reaction was completed.Reaction solution is poured into dehydrated alcohol and is separated out, dry after cleaning 3 times, sieve
Dispense sample.Obtained product carries out haemostatic effect test, and stop blooding duration how many 106.80s, and haemostatic effect is preferable.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by the limit of embodiment
System, other any changes made without departing from the spirit and principles of the present invention, modification, combination, substitution, simplification should be
Equivalence replacement mode, is included within the scope of the present invention.
Claims (8)
1. a kind of method that pure water mutually prepares styptic powder, it is characterised in that the following steps are included:
(1) pre-treatment of starch:
Starch is mixed with acetone and is soaked for a period of time, elutes drying afterwards, the mixed weight ratio of starch and acetone is 1:0.25-
2.5；
(2) gelatinization of starch solution:
After mixing by starch and water dry in step (1), Heat Gelatinization adjusts pH value after cooling；
(3) preparation of cross-linking agent solution:
Crosslinking agent is taken, surfactant and water are selectively added, stirs evenly to obtain cross-linking agent solution；
(4) cross-linking reaction
Cross-linking agent solution is poured into the gelatinized starch of step (2) and is reacted；
(5) cleaning purifying, screening packaging
Reaction solution is dry after being cleaned with ethyl alcohol, screening dress sample.
2. according to the method described in claim 1, it is characterized in that in step (2) weight ratio of starch and water be 1:5-1:30,
PH value 8-11.
3. according to the method described in claim 1, it is characterized in that the weight ratio of starch and crosslinking agent is 5-80:1；Surface-active
The weight ratio of agent and crosslinking agent is 0-1:4-8.
4. according to the method described in claim 1, it is characterized in that the reaction time is 2-6 hours, temperature range in step (4)
50-75℃。
5. according to the method described in claim 1, it is characterized in that crosslinking agent is epoxychloropropane, formaldehyde, glutaraldehyde or 1,4 fourths
Glycol glycidol ether.
6. according to the method described in claim 1, it is characterized in that starch is potato starch, cornstarch or amylopectin.
7. according to the method described in claim 1, it is characterized in that surfactant be Tween 80, span80, polysorbate60,
One or more of span60 and neopelex.
8. according to the method described in claim 1, it is characterized in that surfactant is span80 and polysorbate60 9:1 in mass ratio
The mixture of compounding.
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| CN106955375A (en) * | 2016-12-07 | 2017-07-18 | 凯文蔡司淀粉科技有限公司 | A kind of medical treatment device for including plant polysaccharide stopped blooding for Minimally Invasive Surgery |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1947800A (en) * | 2006-09-29 | 2007-04-18 | 沈晶 | Hemostatic micro-granules and its prepn. method |
| CN101606949A (en) * | 2008-06-19 | 2009-12-23 | 陕西北美基因股份有限公司 | A kind of is the quick hemostasis agent and the preparation technology thereof of primary raw material with high specific surface micro-pore starch |
| CN101982202A (en) * | 2010-11-02 | 2011-03-02 | 华东理工大学 | Medical hydrogel dressings and preparation method thereof |
| CN102139123A (en) * | 2011-03-25 | 2011-08-03 | 杜宝堂 | Method for preparing intra-operative hemostatic material by cross emulsification of plant starch |
| CN102327601A (en) * | 2011-09-26 | 2012-01-25 | 西北大学 | Hemostat for resisting infection and promoting wound healing and preparation method thereof |
| CN102633890A (en) * | 2012-04-22 | 2012-08-15 | 吉林大学 | Surface cross-linking esterification compound modification method of starch nanocrystal |
-
2016
- 2016-02-01 CN CN201610067467.7A patent/CN105597143B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1947800A (en) * | 2006-09-29 | 2007-04-18 | 沈晶 | Hemostatic micro-granules and its prepn. method |
| CN101606949A (en) * | 2008-06-19 | 2009-12-23 | 陕西北美基因股份有限公司 | A kind of is the quick hemostasis agent and the preparation technology thereof of primary raw material with high specific surface micro-pore starch |
| CN101982202A (en) * | 2010-11-02 | 2011-03-02 | 华东理工大学 | Medical hydrogel dressings and preparation method thereof |
| CN102139123A (en) * | 2011-03-25 | 2011-08-03 | 杜宝堂 | Method for preparing intra-operative hemostatic material by cross emulsification of plant starch |
| CN102327601A (en) * | 2011-09-26 | 2012-01-25 | 西北大学 | Hemostat for resisting infection and promoting wound healing and preparation method thereof |
| CN102633890A (en) * | 2012-04-22 | 2012-08-15 | 吉林大学 | Surface cross-linking esterification compound modification method of starch nanocrystal |
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